Verslag Seventh Inter-Agency Meeting, Boedapest,1988-22-10/11 en Sixteenth Session Codex Committee on Methods of Analysis and Sampling, Boedapest, 1988-11-14/19

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Project 505.0060

Normalisatie monsterneming en analyse Projectleider dr W.G. de Ruig

Rapport 89.03 Januari 1989 Verslag Seventh Inter-Agency Meeting, Boedapest,1988-22-10/11

en

Sixteenth Session Codex Committee on Methods of Analysis and Sampling, Boedapest, 1988-11-14/19

dr \-1. G. de Ruig

Goedgekeurd door: ir G.S. Roosje

Rijks-K\o7aliteitsinstituut voor land- en tuinbomo1produkten (RIKILT) Bornsesteeg 45, 6708 PD Wageningen

Postbus 230, 6700 AE Wageningen Telefoon 08370-19110

Telex 75180 RIKIL Telefax 08370-17717

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Overname van de inhoud is toegestaan, mits met duidelijke bronvermel-ding. VERZENDLIJST directeur sectorhoofden coördinatoren afdelingshoofden

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-1

-SANENVATTING

Er wordt een verslag gegeven over:

- Seventh Inter-Agency Neeting, Boedapest, 1988-11-10/11

- Sixteenth Session Codex Committee on Nethods of Analysis and Sampling

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-

-3-VERSLAG VAN:

Seventh Inter-Agency Meeting, Boedapest, 1988-11-10/11

Sixteenth Session Codex Camruittee on Methods of Analysis and Sampling, Boedapest, 1988-11-14/19

INTER-AGENCY MEETING

De Inter-Agency meeting \>lordt traditiegetrom·T voorafgaande aan de CC/MAS vergadering gehouden. Het is een ontmoetingsplaats van organi-saties, die zich bezig houden met de analyse van voedingsmiddelen. Aanwezig waren vertegenwoordigers van CAC, ISO, AOAC, IUPAC, EOQC (Eu-ropean Organization for Quality Control) en van organisaties voor zui-vel (IDF), granen (ICC), suikers (ICUMSA) en fruit juices (1FJU).

Aan de orde k\>~amen o.a. de volgende onden>~erpen.

- Ringonderzoeken. Door de verschillende organisaties werden tal van ringonderzoeken aangekondigd. Omdat sommigen hiervan voor het R1KILT ook van belang kunnen zijn, zijn de opgaven in een bijlage van dit verslag verzameld (Bijlage 2).

- Verbetering van internationale samenwerking op het gebied van genormaliseerde analysemethoden.

- Toepassing van statistische methoden. Hier werd het werk van ISO/TC69 besproken, in het bijzonder de herziening van ISO 5725. Ook ISO 3534:1977 kwam aan de orde.

- Harmonisatie van ringonderzoeken. Een AOAC/IUPAC/ISO \>lerkgroep heeft een concept-"Protocol for the design, conduct and interpretation of collaborative studies'' gepubliceerd. In Nederland (NNI, Zwart) bestond de vrees dat de eindversie van juli 1988 in deze lAM-vergadering zou worden aanvaard en daarmee een officille status zou krijgen. Er waren echter nog een aantal Nederlandse bedenkingen tegen, die weliswaar opgestuurd waren, maar Zwart was er niet gerust op, dat dit commentaar te bestemder plaatse was gekomen. Hij had daarom gevraagd alert te zijn en, indien mogelijk, aanvaarding te voorkomen. Op de vergadering

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-4-bleek het Nederlandse commentaar er te zi.in; het \>lerd zelfs als

voorbeeld voor de andere organisaties gesteld. Commentaar is nog tot december mogelijk en het is de bedoeling de eindversie in mei 1989 te valideren.

(Dit Protocol is ook voor het RIKILT van groot belang; het geeft een stramien waaraan ringonderzoeken zullen moeten voldoen. Eenmaal

geaccepteerd, zal het ongetwijfeld een dwingend karakter krijgen, waaraan het RIKILT en het hele controlerend onderzoek gebonden zal

zijn. Gezien recente ervaringen met de BDR kan een ringonderzoek een cruciale rol spelen in het forensisch onderzoek.

In dit verband ontbreekt o.i. aan het Protocol een paragraaf die de waarde van een ringonderzoek relativeert. Een dergelijke aanvulling is

op ons initiatief thans alsnog opgestuurd door NNI Commissie

390 69 03).

Er werd opgeroepen tot praktische samenwerking bij ringonderzoeken.

- Validering van analysemethoden. Er werd gewezen op een Brits ontwerp

protocol, dat van belang is voor de EEG na 1992. Ook werd aandacht

besteed aan referentiematerialen, o.a. van BCR.

Door mij werd validering door middel van Criteria naar voren gebracht

en uitgelegd aan de hand van foto~s.

- Analysemethoden. De verschillende organisaties presenteren hun

ana-lysemethoden (Bijlage 2).

- Bemonsteringsmethoden. Het belang werd van alle kanten onderstreept. Er is echter nog geen internationaal geaccpteerde genormaliseerde aanpak.

- USSR voorstel voor genormaliseerde methode voor verassing van voedingsmiddelen voorafgaande aan de bepaling van zware metalen. Dit

voorstel zal binnenkort in JAOAC verschijnen. Van verschillende kanten is commentaar binnengekomen. (Gegevens doorgestuurd aan ACON.)

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-5-CC/MAS

Voor een volledig verslag van de vergadering zij verwezen naar het Verslag van de Nederlandse delegatie en het officiële Codex verslag.

Daarom kan hier worden volstaan met enkele persoonlijke impressies. Als gewoonlijk werd ook dit keer een groot deel van de week vergaderd in twee werkgroepen: een Analyse- en een Bemonsteringsgroep. Dit maal heb ik mij aangesloten bij de laatste groep.

Allerwegen wordt de noodzaak van een verantwoorde bemonstering erkend.

Het is dan ook verbazingwekkend, dat er op dit gebied nog zo weinig geregeld is. "He lopen 25 jaar achter". De respons van de Commodity committee's op een oproep van de vorige CC/t-fAS bijeenkomst ~o~as

bedroe-vend. Er ~o~erd daarom gesteld, dat CC/MAS meer leidinggevend moet optreden. Als eerste aanzet ~o~erd daarvoor een stuk opgesteld.

Nederland merkte op dat in de zuivelwereld w~l veel gedaan is aan

(ISO/IDF/AOAC) normen voor bemonsteringsschema's (mede door

activitei-ten binnen het RIKILT).

De analysewerkgroep heeft een document geproduceerd met de actuele situatie ten aanzien van een lange lijst analysemethoden. Een aantal methoden werd (al dan niet tijdelijk) geëndosseerd.

Andere agendapunten waren o.a.:

Er ~o~erd uitvoerig gediscussiëerd over de type-indeling van Codex

methoden van onderzoek. De vraag werd opgeworpen, of een eenvoudige indeling in routine- en referentiemethoden niet voldoende zou zijn. UK zal een ontwerp-richtlijn maken; intussen wordt commentaar van de

regeringen ingewonnen.

Limit of Detection - Limit of Determination. Op eerdere voorstellen

was commentaar binnengekomen; het secretariaat had echter niet de

regeringen geënqueteerd, omdat men vond dat het opstellen van een definitie beter aan deskundigen (IUPAC, ISO, AOAC) kan \o~orden

overgelaten. NL wees in dit verband op een Engelse aanbeveling, waarin

de noodzaak tot twee definities ontkend wordt. Er kon nu verder geen

besluit worden genomen; dit werd doorgeschoven naar de volgende vergadering. Ook de discussie over dit onder,o~erp zal consequenties

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-6-Bij de bespreking van het IAH verslag k,.,am het al even aan de orde, maar bij "Andere zaken" kreeg ik ook in deze vergadering gelegenheid validering van analysemethoden door middel van criteria aan de orde te stellen. Er was behoorlijke belangstelling, ook in de wandelgangen.

Door de voorzitter ,.,erd gesteld, dat chemometrie een opkomende

discipline is, die in de naaste toekomst ook voor de Codex van grote waarde zal blijken te zijn. Wat de criteria betreft, sprak hij uit, dat het vooralsnog zaak is, in de wetenschappelijke wereld hiervoor belangstelling op te wekken en dat hij bereid was persoonlijk hieraan mee te ,.,erken.

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Bijlage 1

Remarks on "Protocol for the design, conduct and interpretation of collaborative studies"

by NNI Commission 390 69 03.

He sametimes notice a tendency to interpret a succesful collaborative study as imp1ying a guarantee for the correctness of a result obtained by the methad studied, irrespective of the nature of the sample

examined.

To prevent the unjustified extrapolation of the results of

collaborative studies to areas neither aimed at nor covered by the study, a cautionary clause should be added, pointing out the

limitation inherent to a collaborative study.

Such a clause could read as follows:

1. A collaborative study gives information about the precision of a method. As such, in most cases it cannot give information about the bias of the method.

2. The results of a collaborative study are valid only for the sampled population, or proven similar ones, in terms of parameters like matrix effects, interfering components, concentratien ranges, etc.

lt does not warrant correctness of the results when the methad is applied to ether populations with different parameters.

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( J

November 1988

INTE R- AG ENCY MEETING

ANALYSIS OF MILK ANO MILK PRODUCTS

INTERLABORATORY STUDIES UNOER IOF/ISO/AOAC AUSPICES Note prepared by lOF General Secretariat

According to the information available·in IDF General Secretariat the foll -owing interlaboratory studies are planned or in,hand in the various !OF/ISO/ AOAC groups of experts

E5 Water content

Total solids in yogurt Total solids in ice cream Total solids in caseins and caseinates (IDF Stanáard 788)

Total solids in cheese and proces~ed

chaase (lOF Standard 4A)

Tota 1 so 1 i ds in· sweetened condensed milk (IDF Standard 15A)

Water content in Butteroil

(lOF Standard 23) ~

.

Water content of dried milk {LOF Standard 26)

Stûdy to be started shortly Study completed: report accepted for publication in Bulletin of lOF Study planned

Study planned

Study completed: report accepted publication in Bulletin of lOF

Study completed: report accepted for publication in Bulletin of lOF

Study planned E8 Nitrate, nitrite, phosphorous, chloride etc ..

Salt content of butter (IDF Standard 12A)

Polyphosphates in cream, evaporated milk and processed cheese (by HPTLC and paper chromatography)

Nitrate in milk powder and whey powder Nitrate in preserved grated cheese (amino-bonded HPLC column)

E9 Lactic acid and lactates Calcium in milk and dried milk

Ell Analysis of caseins and caseinates Ammonia in ammonium caseinates

ElS Heavy metals and ·other elements Tin in canned milk products

Zinc in milk

Study completed: report submitted for publication in Bulletin of IDF Study in hand at present

Preliminary study completed

Pilotstudy completed: full study planned

Study completed: report submitted for publication in the Bulletin of

IDF

Study launched, November 1988 New study planned

Study planned for late 1988 El7 Characterization of d.m. by heat treatment and usage

Cysteine number methad Poor results of study have lead to new approach

Heat class of milk powder-HPLC methad . New study launched August 1988

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Inter-Agency meeting-page 3 E55 continued

Viscosity

E56 Lactulose content

Lactulose in heated milk (HPLC and enzymic methods)

E57 Oxygen in milkfat Photoelectric method

E64 Listeria monocytogenes Detection and enumeration

Study planned

Study completed: submitted for publication in the Bulletin of !OF

Preliminary study launched May 1988

Preliminary studies in hand Reports of interlaboratory studies may be published in the Bulletin of IDF (see, for example, Bulletin of lOF 1986 No 207), Journal of the AOAC, Oeutsche .Lebensmittelrundischau etc. IDF Standard 135A gives guidance on the

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I n t e r - A g e n c y Meeting IDF/ISO/AOAC

Methods of analysis for FAO/WHO Code of Principles

concerning Milk and Milk Products

November 1988

Immediate review of the latest list (in Appendix 2 of 1986 Milk Committee

report) shows the following position. All standard methods are reviewed

5 years after publication todetermine whether they need revision or can

be confirmed.

Product Col lab. FAO/HHO !OF ISO -AOAC

study (!4th Ed) Acid casein ash (fixed) 818:1978 88: 1979 5544:1978 (confirmed) Ammonium caseinate· · ash (fixed) 818: 1978 89:1979 (confirmed) Butter

acid value: free fatty

acid index + 84: 1967 68:1989 1740:1980 16.237-16.239

salt (chloride) + _... 88:1967 12A:1969 1738:1980 16.235

(confirmed)

fat + 89:1978 80: 1977 . 3727: 1977 16:232

refractive index {butterfat) .+ 85:1967 7A:1979 1739:1975 16.240

(confirmed)

sampling 81:1982 508:1985 707:1985 16.012-16.014

solids-not-fat + 89:1978 80: 1977 3727:1977 16.231

total sol i ds .(water) + 89: 1978 80:1977 3727:1977 16.231

Caseins

acidity (fat ac~dity) 826:1982 91:1979 5547:1978

(confirmed) Caseins and caseinates

ash (fixed ash) 824:1982 89:1979 5544:1978

lactose 838:1982 106:1982 5548:1980

nitrogen (protein) 825:1982 92:1979 5549:1978

pH value 837:1982 115:1982 5546:1979

scorched particles 834:1982 107:1982 5739:1983

total solids (water) 822:1982 788:1980 5550:1978

(confirmed) Cheese

chloride + 818:1978 88:1979 5943:1978

(confirmed)

citric acid + 813:1972 348:1971 2963:1974 16/292-16.296'

nitrate and nitrite + 819:1984 84A:1984 4099:1984

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Product

Milk(cont) total solids Milk & foodstuffs

containing milk products lactose (in the presence of other reducing sub-stances

Milk & liquid milk prodijcts

samp1 ing

·-Milk & milk products copper · iron - 3 -Collab. FAO/WHO Study + 829:1982 827:1982 81:1982 + 836:1982 835:1982 scorçhed particles, milk ·

& milk products, caseins

& caseinates sampling (attributes sampling schemes) sampling {general sampling techniques) sampling (variables sampling schemes) Milk,cream & evaporated milk total solids Mi 1 kfat foreign fat foreign fat Milkfat (anhydrous) perodide value rennet casein, &

caseinates ash

Skimmed milk, whey buttermilk

fat

Sweetened condensed milk .fat sucrose tot a 1 so 1 i ds Whey cheese fat 834:1982 821:1982 81:1982 + 829:1982 + 817:1978 + 816;1978 + 820:1978 823:1982 + 832:1982 + 87:1967 + 814:1972 + 830:1982 + 810:1973

lOF ISO AOAC

(14th Ed) 218:1987 DIS 6731 16.032 '79A:1985 OP 5765 508:1985 707:1985 16.001-16.018 76A:1980 5738:1980 25.066-25.071 103A:1986 DIS 6732 107A:19897 5739:1983 113:1982 OP 5583 508:1985 707:1985 16.001-16.005 136:1986 OP 8197 218:1987 DIS 6731 16.032, 16.171 16.189 . 54:1979 3594:1976 28.100 32:1965 3595:1976 28.096 74:1974 3976:1977 not 28/025 90:1979 5545:1978 (confirmed) 228:1985 7208:1984 13C:1987 1737:1985 16.192 35:1966 2911:1976 16.208-16.209 (confirmed) 158:1988 DIS 6734 not 16.203 59A:1986 18(~è~~)2 16.285

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'')' ·I

.

Since 1884 ML/ 140/88 agenda item 10.2 milk etc i ces

Association of Official Analytica} Chemists

1111 North 19th St. Suite 210 • Arlington. VA 2220Y USA • 70.'-3- 522 -.130.'-32 Postbus 153 • 6720 AD Bennekom • The Netherlands • + 31 · x:H~9-IX72:J

Seventh Interagency Meeting

Budapest ,Hungary,lO and 11 Nov.l988

Contribution by AOAC on Methods of Analysis,agenda item 10 methad

Babcock + ether extr. of fat in milk lnfrared analysis of milk

Calcium Phosphorus and Magnesium in Cheese

HPLC for Iodide in mil~

see IDF/ISO/AOAC methods

see IUF/ISO/AOAC methods

status adopted adopted review review review 10.3 edible

10.5 methods for infant formula :FOA and IFC studies

f.For dietaryPhase I-s and II-s for soybased formulations

USBS review 10.6 fruit juices 10.8 meat 10.9 sugars 10.12

Quinic,malic,Gitric acids in éranberry juice cocktail

and apple juice adopted

L-i·ialic/total malie acid ratio; in dateetion of econornic

adulteration of apple juice review

adulteration of apple juice and orange juice review glycerol in wine and grapefruit juice by HPLC review

FSIS study on fish in Frankfurters review

Saxtee fat analyzer for total fat content in meat review

Sucrose in molasses by HPLC:

Sugars in ~yrups and molasses

review review

microbiology Filth in flour(corn) flotation·method Filth in eggs and egg products

adopted

adopted adopted Filth in mushrooms

Bird and insect excrements on food and containers

(TLC methad for uric acid)

Aerobic plate count,E coli,coliforms,Staph.in fro:en

chilled precooked ar prepared foods Thermophilic bacterial spares in sugars

Virus in beef(ground)

Sporeformers in lew-acid canned foods

Poliovirus in oysters

Sa~onella in foods(DNA hybridization method)

Salmonella in lo1t1-moisture foods( enzyme im1aunoassay)

-2-adopted adopted adopted adopted adopted adopted adopted adopted

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I U P A C COMMISSION VI.3 - OILS, FATS ANO DERIVATIVES WORKING PROGRAMME FOR 1987 - 1988

WG No. 3/78 3/79 ad hoc 1/80 1/83 2/83 1/85 2/85 1/87 2/87 3/87

Title of Working Group

Determination of benzo-a-pyrene Determination of mineral oil

(middle fraction)

Determination of the colour of lecithins

Oetermination of n-3 and n-6 fatty acids in vegetable oils

Determination of lead

Oetermination of triglycerides according to their ECN's

Oetermination of polymerized tri-glycerides

Determination of phospholipids in commercial lecithins

Oetermination of total satd., total trans, and n-3 & n-6 fatty acids animal oils and fats

Oetermination of benzo-a-pyrene

Principle of methods column and HPLC

capillary glc

Lovibond (auto) and speetrometry capillary glc

AAS (graphite furnace) reversed phase HPLC gel-permeation HPLC HPLC capillary glc column & HPLC Future work:

Four new Working Groups will be organized:

- trans-isomer content determination to control cold pressed oils - phosphorus content by AAS

solvent residues (different types) in vegetable oils

- revision of the methods for acid value and peroxide value determination

--J~

l·

~

Co-ordinator (assistant) P Hendrikse G Osterman P Hendrikse R Ohlson (A Nasner) A Dieffenbacher (J Beare-Rogers) P Hendrikse J P Wolff CF Mordret) J P Wolff (F Mordret) J Beare-Rogers (A Nasner) A Oieffenbacher (J Beare-Rogers) P Hendrikse (G Ostermann) <::?

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~~ _t~ ~

.

I

i u r" ,... \" \... U 1•11'll ~ ~ 1 U N I ' " I" U U U l. H t M 1 S r K Y

•

C u r r e n t P r o j e c t s Updated

&

Revised : May 1986

WORKING GROUP PROJECT P R 0 J E C T TITLE · FIRST CO-OPTED STATUS EXPECTED

NUMBER COORDINATOR ORGANISATIONS COMPLETION

DATE Mycotoxins 11/81 Check-sample survey for mycotoxins Ca stegnare IARC On-going 1985

Aflatoxin B₁~ B₂~ G₁

&

_G2

in M~ize and Peanut Meal

Aflatoxin Mr. in Milkpowder Ochratoxin A in Wheat flour

30/85 Collaborative Study Krogh · AOAC On-going 1987

Ochratoxin A in Barley~ Maize and Pi g-1 i ver Comparison of TLC-Separation/ UV-Determination and

HPLC-separation/UV-Determination-Methods

31/85 Collaborative study of an HPLC methad Park AOAC On-going 1987

for determination of Aflatoxins in Ground nuts and C:ereal grains

35/86 Spectro-analytical parameters Steijn IUFOST On-going 1987

of Fusarium toxins IUMS

ISPP

38/* Collaborative S}udy Kubacki _ISO Submitted . 1987

Patulin in Apple Juice for CFC

Camparisen of two methods with HPLC- approval

Separation and UV-Oetermination

37/86 Limits and Regulatieris for Mycotöxins Park IARC On-going 1988

tn foods and feeds WHO/FAO

Joint Mycotoxin Committee of ."_

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~

... .

.

Aquatic

41/*

Biotoxins Production of a world-wide directory Krogh WHO/FAO Submitted 1987

on laboratories conducting aquatic for CFC

biotoxin analysis approval

Elemental

Analysis 28/85 Collaborative Study Vaessen

-

On-going 1986

Selenium in Milk-Powder

& Pig-Liver Wet-digestien and Determination by Fluoreszenz-photometry

29/85 Collaborative Study Vaessen

-

On-going 1986

Sodium & Potassium in Milk-Powder & Infant Foods Wet-Digestien and Determination by Atomie Absorbtien Speetrometry

34/86 Collaborative Study Vaessen

-

On-going 1987

Magnes i urn & Cal c i urn in Mil k -Po'11der & Infant Foods Wet-Digestien and Determination

by Atomie Absorbtien Speetrometry

Nitrosamines 5/81 Feasability and Collaborative Study Castegnaro

-

On-going 1986

Total N-Nitrosamines in Urin and Saliva HBr-Pre-Treatment and direct Thermal

Electron Analycer-Determination

39/* Collaborative Study Polloek EC Submitted 1987

Volatile N-Nitrosamines in Rubber- AOAC for CFC

Nippels and Pacifiers IARC approval

Comparison of FDA-Method: CH₂Cl 2-Extraction/Determination by

GLC/TEA and BGA-Method: Salviasimulant-Extraction/Determination by GLC/TEA

40/* Check-sample survey Castegnaro IARC I bid 1987

Non-volatile-N-Nitrosamines in Malt & Beer·

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I

;

·

\; .·~ / Natural Toxicants Halogenated Hydrocarbons Environmental Contaminants 36/86 32/85 33/85

Natural Toxicants in Foods-Phase I

Inventory of institutes, methods

&

problems.

Current knowledge/state of the art

Chromatographic separation of 135

chlorinated dibenzo-p-Oioxin and -Furan-Isomers

GL-Capillary-Chromatography and Electron Capture Detector

Determination of Retention-Indices and Oetection~Response Factors Feasability Study

Evaluation of PCB-Quantification in Foods and other biological samples Battaglia Conacher Conacher (3)(...)> " On-going 1987 On-going 1987 On-going 1987

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f()

ISO TC 93

Collaborative studies planned 1989

1. Determination of mono, di, tri and oligo aaccharidea in staroh hydralysis producta (HPLC)

Contact: Mme Duhau AFNOR

Tour Europe

92080 Paria La Defenee Cedex 7

2. Determination of acetyl content (degree of eubetitution)

of ataroh aoetatee

2.1. Saponification (non-epeoific) methad 2.2. Gas chromatographio methad

2.). Enzymatic methad Contact: i 0 Mr R·. ·Zwart NNI P.O.Box 5059 NL 2600GB Delft

J.

Determination of adipyl oentent (degree of aubetitution) of staroh adipatee-(GLC)

Contact:

as

2

4. Determination of oarboxyl value of oxidised atarches -

titra-tion methad

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\ \ Terminology ISO 5526:1986 Sampling ISO 2170:1980 CFD :1985

METHODS OF TEST FOR CEREALS, CEREAL PRODUCTS AND PULSES

ISO/TC 34/SC 4 "Cereals and pulses" 1988. November

CEREALS AND PULSES

Cereala, pulsas and other food grains - Nomenclature Trilingual edition

First edition

Careals and pulsas -Sampling of milled products Second edition

Thousand. karnel weight ISO 520:1977

CFD :1983

Ash content ISO 2171:1980

CFD :1986

Cereals and pulses - Determination of ~he mass of 1 000 grains

First edition

Cereals, pulsas and derived products - Determinatlon of ash Second edltion.

Extraneous matter (Fllth test)

i

ISO 6639-1:1986

ISO 6639-2:1986

Careals and pulsas - Determination of hidden insect lnfestatlon

-Part 1: General principles First edition

Careals and pulses - Determination of hidden insect infestation

-Part 2: Sampling First edition

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' Terminology ISO 5527-1:1979 DP 9228 Sampling ISO 950:1979 CFD :1985 I ISO 6644:1981 CFD :1988 Moisture content ISO 711:1985 ISO 712:1985 ISO 7700-1:1984 Total fat ISO 7302:1982 CFD :1987 Enzyme activity ISO 3983:1977 ISO 30.93:1982 CFD :1987 DP 7973 - 3 ~

CEREAI.S AND CEREAL PRODUCTS

Careals - Vocabulary - Part 1 Bilingual edition

Flrst editlon, under re vision

Careals - Terrus and definitions relatlng to grain drylng

Cereals - Sampling (as graln) First edition

Careals and milled cereal products - Automatic sampling by mechanical means

First editlon.

Cere.als and cereal products - Determinatio.n of motsture content (Basic raferenee method)

Second edition.

Careals and cereal products - Determination of motsture content (Routine raferenee method)

Second edition.

Check of the calibration of motsture meters - Part 1: Motsture meters for careals

First edition

Cereals and cereal products - Determination of total fat content First edition

I I

Cereals and cereal products - Determination of alpha-amylase activity

Flrst edition, under revisi9n

Cereals - Determination of falling number First edition

Cereals and milled cereal products - Determination of amylograph viscosity

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I') .J ISO 6820:1985 Gluten ISO 6645:1981 CFD :1988 ISO 5531:1978 CFII>- :1988 DIS 7495 - 5 -WHEAT FLOUR

Wheat flour and rye flour - General guldance on the draftlng of

bread-making tests

First edition

Wheat flour - Determlnation of dry gluten

First edltion.

Wheat flour - Determination wet gluten

Flrst edition

Wheat flour - Automatic determinatlon of wet gluten by mechanica!

means Physlcal Dough Testing DIS 5530-1 DIS 5530-2 DIS 5530-3 ISO 5530-4:1983 Vltreousness ISO 5532:1987 Sensory analysis ISO 7304:1985

Wheat flour - Physical characteristlcs of doughs - Part 1 :·

Determinatim of water absorption and rheological properties

using a farinograph

Wheat flour - Physical characteristics of doughs - Part 2:

Determinatlon of rheological properties using an extensograph

Wheat flour - Physical characteristlcs of doughs - Part 3:

Determination of water absorption and rheological properties

using a valorigraph

.

Wheat flour - Physical characteristlcs of doughs - Part 4:

Determination of rheological properties using an alveograph

First edition, under revision.

DURVMWHEAT

Durhm wheat - Determination of proportion of non-wholly

vitreous grains (Reference method)

Second edition

Dururn wheat sernolinas and alimentary pasta - Estlmation of

cooking quality of spaghetti by sensory analysis

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[ {1 IVj t Cj d ó'- I I -I I

/)~

(-Lt

Nordisk Metodikkommitté för Livsmedel

Generalsekretarlatet

NORDIC COMMITTEE ON FOOD ANALYSIS (NMKL) c/o Technical Research Centre of Finland Food Research Laboratory

SF-02150 ESBO FINLAND

To the organ1zat1ons part1c1pat1ng in the Inter-Agency Meeting

Esbo, 30 December 1987

ANNOUNCEMENTS OF NMKL COLLABORATIVE ANALYTICAL STUDIES OF METHOOS OF ANALYSIS

ENCL

POSTADRESS

Please find enclosed information on collaborative

analytical studies of methods of analysis scheduled for spring 1988 within the Nordie Commfttee on Food Analysis (NMKL):

*

Fat. Determination in meat and meat products according to SBR (Schmid-Bondzynski-Ratslaff)

*

Campylobacter jejuni/coli. Detection in foods

*

Aspartame and diketopiperazine. Liquid chromatographic determination

* Metals. Determination by atomie absorption

For your information a recent list of all published NMKL

-· methods is enclosed and also a news-sheet presenting recently publfshed NMKL methods.

NMKL wishes everyone a Happy New Year 1988.

Si ncerely ,·

~ttÀ&

Harriet Wall in Secretary General

BANKFÖRBINDELSE

NORDISK METOOIKKOMMITIE FÖR LIVSMEDEL

c/o Stalens leknlska forsknlngscentral

TELEFON Nat. (90) 4561 Int. +358-o-4561 TELEX 122972 vttha st POSTGIRO 2238-9 Livsmedelslaboratorlet SF-02150 ESBO, FINLAND

(25)

r·;.

Nordisk Metodikkommitté för Llvsmedel

., ~~ . Generalsekretariatet Date Or9anization Analyte Cammodi ty Principle of Methad . Approx. Concentratien-Range

No. of Samples per Participant Purpose of Trial .. Month of Distribution of Samples , I .

Time Allowed .for ~nalysis

of Samples (in Week~) .

Expected Date of Report Contact - Address for trials open to Other Participant~ ·

POSTADRESS

NORDISK METODIKKOMMITIE FÖR LIVSMEDEL c/o Slalens leknlska lorsknlngscentral

Llvsmedelslaboratorlet SF-02150 ESBO, FINLAND

30.12.1987

Nordie ·Committee on Food Analysis

Fat (accordin9 to Schmid-Bondzynski-Ratslaff, SBR) Meat and meat products

SBR: Fat extraction with a mixture of ether and petroleum ether after treatment of food with hydrochloric acid and addition of alcohol. Distillation of solvent and wei9hing of residue 2-50 9 fat/100 9

12

Revision of existin9 NMKL methad no 88 Fat.

Determination in meat and meat products accordin9 to SBR (Schmid-Bondzynski-Ratslaff). (Samples to be analysed with bath no 88 and with proposed revised method)

January 1988

4.

.

30.5.1988

Trial not open to others (sufficient number of laboratories within Nordie countries has already reg i stered) TELEFON Net. (90) 4561 Int. +358-Q-4561 TELEX 122972 vtlha ar BANKFÖABINDELSE POSTGIRO 2238-9

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Nordisk Metodikkommitté för Livsmedel ~ Generalsekretariatet Date Organization Analyte Commodi ty Principle of Method Approx. Concentration-Range

No. of Samples per Participant

Purpose of Trial

30.12.1987

Nordie Committee on Food Analysis Campylobacter coli/jejuni

Foods (chicken liver)

Enrichment in broth containing antibiotics,

plating on solid selective medium, incubation at 42°C for 48 h in microaerophilic conditions,

· biochemical verification

0-1000 per gram

8

To validate published proposed NMKL method nr 119 (1986) "Campylobacter jejuni/coli. Detection in

foods11

Month of Dfstrfbution of April 1988. Pretest includfng 3 samples scheduled

Samples. for March 1988

Time Allowed for Analy$iS 3

of Samples (in Weeks)

Expected Date of Report 31.7.1988

Contact - Address for trials Trial not open to partfcipants outside the Nordie

open to Other Participant~ countries due to problems with shipping of

biological tissues POSTADRESS

NORDISK METODIKKOMMITIE FOR LIVSMEDEL

c/o Slalens leknlska lorsknlngscenlral Llvsmedelslaboralorlel

SF-Q2150 ESBO, FINLAND TELEFON Nel. (90) 4561 Inl. +358-Q-4561 TELEX 122972 vllha si BANKFÖRBINDELSE POSTGIRO 2238-9

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Nordisk Metodikkommitlé för Livsmedel , - Generalsekrelarialet Date Organization Ana lyte Commodity Principle of Method Approx. Concentration-Range

Purpose of Trial

Month of Dfstribution of sa.mp 1 es ·

Time Allowed for Analysis of Samples (in Weeks) Expected Date of Report Contact - Address for trials open to Other Participants

POSTADAESS

NORDISK METODIKKOMMITIE FCR LIVSMEDEL c/o Slalens leknlske lorsknlngscenlrel

llvsmedelslaborelorlel SF--()2150 ESBO, FINLAND

30.12.1987

Nordie Commfttee on Food Analysis Aspartame and diketopfperazfn (DKP) Beverages. marmalades

Dilution. ffltration. LC separation. UV detection at 214 nm Beverages 0-600 mg aspartame/kg. 0-200 mg DKP/kg ~~ r~armalades 0-1200 11 • 0-200 11 20 Nordie legislation February 1988 2 . 30.5.1988 Astrid Nordbotten Arne Vidnes

The National Quality Control Authorfty for Processed Frufts and Vegetables

Gladengveien 3 B P.O.Box 6399 - Etterstad N-0661 OSLO. Norway TELEFON Net. (90) 4561 Inl. +358--()-4581 TELEX 122972 vttha el BANKFÖRBINDELSE POSTGIRO 2238-9

(29)

\ t

Nordisk Metodikkommitté för Livsmedel Generalsekretarlatet Date Organization Analyte Gommodi ty Principle of Method Approx. Concentration-Range

Purpose of Trial

Month of Distribution of Samples

Time Allowed for Analysis of Samples (in Weeks)

I .

30.12.1987

Nordie Committee on Food Analysis Metals. Pb, Cd, Cr, Cu, Fe, Zn Foods generally

Dry ashing at 45ooc, addftfon of HCl, evaporation to dryness, dissolution in HN0 ₃, flame or graphite furnace atomie absorption spectrophotometry

measurement

Down to limit of determination as determined.in the laboratory according to method

6

To validate method for the needs of international legislation

March 1988 (instrumental pre-testing performed in December 1987)

4

Expected Date of Report 30.9.1988

Contact - Address for trials Trial not open to others. A sufficient number (19)

open to Other Participants of laboratorfes within the Nordie countries has

already registered

POSTADRESS

c/o Stalens teknlska loraknlngscentral Llvsmedelslaboralorlel SF-()2150 ESBO, FINLAND TELEFON Nol. (90) 4561 Int. +358--o-4561 TELEX 122972 vttha al

BANKFÖRBINDELSE

POSTGIRO 2238-9

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NORDIC COMMITTEE ON FOOD ANALYSIS

c/o·Technica1 Research Centre of Finland

Food Research Laberatory

SF-02150 ESBO FINLAND P U B L I S H E 0 M E T H 0 D S No 1 2 3 4 5 6 7 8 9 10 Name

Determination of boric acid (H₃B0₃)

Benzoic acid (C₆H₅COOH), determination of

Determination of salicylic acid {C₄H₆0HCOQH 1.2)

Chemical methods for the detection of in~ff~cient

cleansing of cups, dishes and plates · '

Total number of microbes. Oetermination with the swab method or contact plate method on utensils in contact with food

Nitrogen. Oetermination in foods and feeds accord-i ng to Kj el dahl

Ash. Oetermination in grain and flour Determination of formic acid (HCOOH) Reduction tests for milk

Gravimetrie determination of fat in milk, cream, condensed and dried milk

11 c a n c e 1 e d (replaced by No 107, 108, 109 and 110)

12 c a n c e 1 1 e d

13

14

Determination of motsture content of grains and of certain grain products

Additions and corrections, No 13 Determination of moisture in bread

I 15 c a n c e 1 1 e d 16 c a n c e 1 1 e d 17 c a n c e 1 1 e d 18 19

Sulphurous acid (S0₂). Determination in foods

Additions and corrections, No 18

Determination of flourine in calcium compounds and

cereals wit~ added calcium compounds

1 December 1987 Year of publication 1950 1979 1968 1962 1987 1976 1987 1966 1953 1977 1977 1983 1953 1970 1980 1955 . 3rd Ed. 2nd Ed. 2nd Ed. _. _. 4th Ed. 3rd Ed. 2nd Ed. 2nd Ed. 2nd Ed. 2nd Ed. 2nd Ed.

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2

20

21

Methods for microbiological examinations of butter Determination of calcium in cereals

22 c a n c e 1 1 e d (replaced by No 116}

23 Moisture and a~h. Determination in meat and meat products 24 c a n c e 1 e d 25 c a n c e 1 1 e d 26 27· 28

Pasteurization control of milk, cream and whey -Determination of phosphatase activity

Determination of the total plate count in milk, cream and ice cream products by means of the plate count method

Analytica1 determination by weight of the total so1ids of tomato purée

29 c a n c e 1 1 e d 30 31 32 33 34

Determination of copper in foods

Isolation and identification of waterso1uble, syn

-thetic colouring matters

Isolation and identification of oil-soluble, synthetic

c~louring matters

Identification of sugars by paper chromatography Sampling of grains, milling products, and starch products 35 c a n c e 1 1 e d (replaced by No 112} 36 c a n c e 1 1 e d 37 38 39 40 41

Fermentation test for non-specific, qualitative detection of preservatives in foods

Acid value. Determination in fats

Iodine value. Determination in fats (Wij's method) Determination of fat content in milk by the Gerber method

Determination of organic combined halogen in bever-ages, fruit juices, and marrnalade

42 c a n c e 1 ~ e d (replaced by No 123}

43 Determination of mono and disaccharides in pure aqueous solutions (according to Potterat

&

Eschmann}

1982 1955 1974 1985 1982 1958 1958 1959 1959 1981 1974 1961 1975 1972 1961 1961 1962 2nd Ed. 2nd Ed. 3rd Ed. 2nd Ed. 2nd Ed. 2nd Ed. 3rd Ed. 2nd Ed.

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..

44 45 46 47 48 49

Coliform bacteria. Determination in foods

Determination of the peroxide value of pure fats, butter and margarine

Determination of lead in foods

Method for determining the keeping quality of ster-ilized canned food

Determination of p-hydroxybenzoic acid esters Determination of nitrite

I Unspecific tit~imetric routine method for the

deter-mination of nitrite in "nitrite salt" and "nitrite saltpetre"

11 Determination of nitrite in "nitrite salt" and nitrite

salpetre", and in meat, fish, and brine

50 51 52 53 54 55 56 57 58 59 60 61

Quantitative determination of the antioxidants BHA

(3-tert-butyl-4-hydroxyanisole) and BHT (3.5-di-tert

-butyl-4-hydroxytoluene) in fats Determination of cadmium in foods Starch. Determination in meat products

Preparation and clarification of extracts for sugar determination

Determination of formaldehyde in foods

Determination of net content and drained weight of preserved fruits and vegetables

Determination of the number of sulphite-reducing clostridia in foods

Determination of the total content of phosphorus in foods

Determination of' zinc in foods

Mikrobiological examination of fully preserved canned foods

Preservatives. Detection by TLC (proposed method)

Determination of sorbic acid (CH₃CH=CH-CH=CHCOOH)

according to the thiobarbituric acid method (TBA method) 62 c a n c e 1 1 e d (replaced by No 125) 3 1975 1962 1962 1963 1963 1963 1963 1963 1984 1964 1964 1980 1980 1965 1965 1978 1987 1972 2nd Ed. 2nd Ed. 2nd Ed. 2nd Ed. 2nd Ed. 2nd Ed. 2nd Ed.

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4

Determination of oxalic acid

64 Determination of solids in canned kale and spinach 65 c a n c e 1 1 e d 66 67 68 69 70 71 72 73 74 75 76 77 78 79 80 81 82

Determination of Staphylococcus aureus Determination of Bacillus cereus in foods Determfnation of fecal streptococci in foods

Detection of the antioxidant DPPD (N' ,N-diphenyl-p-phenylenediamine)

Tomato purée and tomato paste. Refractometrie determi-nation of soluble dry matter

Salmonella bacteria. Detection in foods

Biphenyl. Determination in citrus fruits, marrnalade of citrus fruits, and in apples and pears

o-Phenylphenol. Determination in citrus fruits, marrnalade of citrus fruits, and in apples and pears Psychrophilic bacteria. Oetermination by the plate count methad

Psychrophilic bacteria. Determination by measuring the growth rate of bacteria during cold starage (tentative method)

Condensed phosphates (polyphosphates).

Identifi-cation in meat products, etc. by paper chromatography a-AmYlase activity. Determination in cereals and

cereal products

Lactose. Oetermination in milk chocolate

Botulinum toxin. Determination in foods and serum Clostridium botu1inum. Detection in foods

Paralytic shellfish poison. Biological determi-nation in the common mussel and other bivalves Methylmercury compounds. Determination in fish Corrections, No 82

83 c a n c e 1 1 e d

84 Dodecyl gallate (DG), octyl gallate (OG), n-propyl gallate (PG) and nordihydroguaiaretic acid

(NOGA). Detection in fat. TLC-method 85 c a n c e 1 1 e d (replaced by No 104) 1967 1967 1980 1982 1978 1969 1969 1985 1970 1970 1970 1970 1970 1970 1970 1979 1979 1986 1972 1980 1984 2nd Ed. 3rd Ed~ 2nd Ed. 2nd Ed. 2nd Ed.

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8.6 Aerobic micro-organisms. Enumeration at

3ooc

in meat and meat products

87 c a n c e 1 1 e d (replaced by No 115) 88 89 90 91 92 93 94 95 96 97 98 99 100 101 102 103 104 105 106

Fat. Determination in meat and meat products accord-ing to SBR (Schmid-Bondzynski-Ratslaff)

Chloride. Determination in meat and fish products

Corrections, No 89

Aflatoxin. Determination in peanuts and peanut products

Corrections, No 90

Pretreatment of solid foods for microbiological examination (dept-infected and surface infected) Mould count. Determination in tomato products Glucose. Determination of the total amount in meat products after hydralysis

Extraction of heavy metals, especially from enam-elled articles and glazed ceramic articles

Clostridium perfringens - Determination in foods Bacteriological examination of fresh and frozen fish and fish products

Vibrio parahaemolyticus. Detection in foods (tenta-tive method)

Mould. Determination in foods (proposed method) Histamine. Determination in fish

Nitrite and nitrate. Determination in meat products, brines, and saltmixtures (tentative method)

Detection of aflatoxins with minicolumn

Detection of saccharin, cyklamate och dulcine in soft drinks

Benzoic acid and sarbic acid in foods. Quantitative determination by gas chromatography

Measuring of water activity with a polyamide fila-ment hygrometer

Determination of coliform bacteria in foods using pre-incubation (proposed method)

Determination of ochratoxins in barley by thin layer chromatography 5 1986 1974 1974 1986 1975 1980 1975 1976 1978 1979 1985 1980 1982 1987 1981 1982 1982 1984 1984 1984 1984 1984 2nd Ed. 2nd Ed. 2nd Ed.

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6 107 108 109 110 111 112 113 114 115 116 117 118 119 120 121 122 123 124 125

Milk and cream. Determination of titratable acidity (routine method)

Milk and milk products. Determination of ash Milk, cream and preserved milk. Determination of chloride, argentometric titration

Milk and milk products. Determination of total solids (water). Gravimetrie method

Folate, biologically active, in milk and milk

products. Microbiological determination with

Lacto-bacillus casei

Arsenic in foods and food additives. o'etermination

by molybdenum blue method

Calcium and magnesium. Determination by complexa-metrie titration

Isolation and identification of watersoluble, syn-thetic colouring matters {proposed method)

Tin. Quantitative determination of the total content in food. Spectrophotometric determination with quer-cetin

Iron. Photometric determination in food Yersinia enterocolitica. Detection in food Histamine. Thin-layer chromatographic screening method {proposed method)

Campylocater jejuni/coli. Detection in foods {proposed method)

Benzo(a)pyrene. Fluorescence spectrophotometric

determination in smoke preparations (proposed method) Antibacterial substances. Detection by a

micro-biological method in kidney and muscle from slaughter

animal~ {propose~ method)

Saccharin. Liquid chromatographic determination in beverages and sweets

Cyclamate. Spectrophotometric determination in food Bensoic acid, sorbic acid and p-hydroxybenzoates. Liquid chromatographic determination

Thermotolerant coliform bacteria. Determfnation in

foods after pre-incubation

1984 1984 1984 1984 1985 1905 1985 1985 1985 1985 1987 1986 1986 1986 1987 1987 1987 1987 1987 (

..

2nd Ed

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1.1

7

R E P 0 R T S

No 1 Statistical Evaluation of Results from Quantitative 1983 2nd Ed

Microbiological Examinatfons

No 2 Stikpr,Sveplaner til mikrobiologi.sk unders0gelse af 1983

levnedsmidler - Principper for pr0veudtagning og praktisk udf,Srelse (In Danish only)

No 3 Kvalitetskontroll av arbetet p~ livsmedelslaboratorier 1983

(Minisymposium 1982-08-24, Esbo, Finland) (In

Scandi-navian languages only)

Nr 4 Fysisk-kemiske h·urtigmetoder til levnedsmiddelanalyse 1986

(l~inisymposium 1985-09-03, Ärhus, Danmark) (In Danish

only)

Nr 5 Handbok för mikrobiologiska laboratorier - Handledning 1987

för intern kvalitetskontroll av analysarbetet (In Swedish and Finnish)

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THE NORDIC COMMITTE ON FOOD ANALYSIS

Nordisk Metodikkommilté för Livsmedel Generalsekretariatet

President

Professor Niels Skovgaard .

Royal Veterinary and Agricultural University Institute of Veterinary Hygiene and

Microbiology Bülowsvej 13

DK-1870 FREDERIKSBERG C

DEN~1ARK

The Danfsh Natfonal Cornmfttee Chairman

Professor Niels Skovgaard

Royal Veterinary and Agricultural University Institute of Veterinary Hygiene and

Microbiology Bülowsvej 13

DK-1870 FREDERIKSBERG C .

DENMARK

The Finnfsh Natfonal Commfttee Chairman

Dr Heikki Pyysalo

Finnish Customs Labaratory Teknikvägen 13

The Icelandfc National Commfttee Chairman Mr Franklin Georgsson, M.Sc. Hollustuvernd rikisins Skipholti 15 IS-105 REYKJAVIK I GELAND

The Norwegfan Natfonal ,Commfttee

Chairman Dr Bjarne Aalvik Dept of Health Engen 39 N-5000 BERGEN NORWAY

The Swedish Natfonal Commfttee

Chai n:ldll

Professor Lembitu Reio

National Food Administration Nutrition Labaratory Box 622 S-751 26 UPPSALA SHEDD~ December 1987 Secretary General

Ms Harriet Wallin, Lic. Ph. Administrative Assistant Ms Eva Fredriksson

Technical Research Centre of Finland Food Research Labaratory

Sec;retary

Ms Eeva-Liisa 0stergaard, M.Sc (Agr) National Food Agency

M~rkh~j Bygade 19 DK-2860 S@BORG DENMARK

Secretary

Ms Thea Sipiläinen-Malm, M.Sc. (Eng) Technical Research Centre of Finland Food Research Laboratory

SF-02150 ESBO FINLAND Secretary Ms Hulda Olafsdottir Islenska matv~larannsoknanefndin Hollustuvernd rikisins Skipholti 15 IS-105 REYKJAVIK I CE LAND Secretary

Mr Arne Vidnes, M.Sc. (Eng)

The National Quality Control Authority for Fruits and Vegetables

Box 6399, Etterstad N-0604 OSLO 6

NORWAY

Secretary

Dr Bonny larsson

National Food Administration Food Labaratory

Box 522

S-751 26 UPPSALA

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I. '/ _{l ,}

Nordisk Metodikkommitté för Livsmedel Generalsekretariatet

NEW NMKL-METHODS

POSTADRESS

The followfng efght methods of analysfs for food have been publfshed by the Nordie Commfttee on Food Analysfs fn 1987 and are avaflable through NMKL's office 1n Finland:

*

Ash. Determfnatfon fn grafn and flour (NMKL no 7, 2nd ed)

This method, which replaces the first edition of the method pub-lished in 1952, has been collaboratively studied. Kaj Michaelsen (Denmark) was responsfble for the study, and Claus Bren~e (Oenmark) has assisted NMKL in working out the ffnal text.

*

Preservatfves. Detectfon by TLC. Proposed method (NMKL no 60, 2nd Ed)

NMKL no 60 (1987) rep la ces the fi rs t edit i on of no 60 pub 1 i shed in 1967 and has been elaborated first by Astri Rogstad (Norway) later by lngegerd Beekman (Sweden). Si nee the method fn fts present form has not been subjected to a collaboratfve study, ft fs published as an NMKL proposed method. A 11 users are f nv i ted to submi t comments on the performance of thfs proposed method.

*

Mould. Determfnatfon tn food. Proposed method (NMKL no 98, 2nd ed)

This proposed method has been prepared by botanist Kerstin .S.ker-strand at the National Food Administratfon in Uppsala, Sweden. Note that this method replaces the ffrst edition of no 98 from 1980:

'Mould. Determination in cereals and cereal products'.

*

Yersfnfa enterocolftfca. Detectfon fn food (NMKL no 117, 2nd ed)

The first edition of this method was issued fn 1986 as an N~1KL pro-posed method. Subsequently, Georg Kapperud and Truls Nesbakken (Nor-wegian Col:lege of Veterfnary Medicine) conducted a collaborative study of the method. The second edition of the method has been re-vised according to experience gained durfng the fnterlaboratory study; . ft includes new instructfons for biochemical and serological characterfzation of suspected Y. enterocolitfca colonies.

*

Saccharfn. Lfqufd chromatographfc determfnatfon tn beverages and sweets (NMKL no 122)

An LC method for the determinatfon of saccharin has been collabora-tively tested. Anna-Maija Sjöberg at the Food Research Laboratory of

NORDISK METODIKKOMMITIE FÖR LIVSMEDEL

c/o Slalens leknlska forsknlngscenlral

TELEFON Nat. (90) 4561 Int. +358-o-4561 TELEX 122972 vttha st BANKFÖRBINDELSE POSTGIRO 2238-9 Llvsmedelslaboraloriet · SF-Q2150 ESBO, FINLAND

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the Technical Research Centre of Finland coordinated the study and the collaborative study report appeared in the 1987 January/February edition of the Journal of the Association of Official Analytical Chemists (JAOAC 70(1987)58).

*

Cyclamate. Spectrophotometrfc determinatfon fn foods

(NMKL no 123)

NMKL no 123 was developed to replace the gravimetrie NMKL method no 42 from 1972. Anna-Maija Sjöberg at the Food Research Labaratory of the Technical Research Centre of Finland arranged the collaborative study of the method. This showed the relative standard deviation for repeatabil ity to be 4.1 % for soft dri nks and 3.2 % for jams. The corresponding reproducibility parameters were 6.7 and 4.4 t. respec-tively. The study report appears in the 1987 May/June edition of the Journa 1 of the Associ a ti on of Offi ei a 1 Analytica 1 Cheni sts (JAOAC 70(1987)588).

*

Benzoic acfd, sorbfc acid and p-hydroxybenzoates. Liquid

chroma-tographic determinatfon (NMKL no 124)

Chemist Bar~ro Halén of the National Food Agency. Uppsala, Sweden

has developed this method and arranged its collaborative testing •.

The test included the sample matrices mayonnaise. fish, cheese and apple juice. A total of sixteen samples with. varying analyte levels and combinations were analyzed in eleven laboratories. The statisti-cal evaluation revealed no interlaboratory variation for any of the five preservatives.

*

Thermotolerant co11form bacterfa. Determfnatfon in foods after

pre-incubatfon (NMKL no 125)

This new method which replaces former NMKL method no 62 (1966) is applicable to all types of food products with the exception of fish products. It was especially developed to obtain a more reliable determination of "stressed" or sublethally injured col iform bacte-ria, which will not grow in violet red bile agar without suitable

pre-incubation. Frits Vagn Jensen and Bj~rn Fredebo Thomsen in

Oen-mark prepared the revised method •

. ·ORDERING UF ·METHODS

All N~·1KL methods are pub 1 i shed in a Scan di navi an 1 anguage (Dan i sh, Norwegian or Swedish) and in English. Since 1985 all new methods are also available in a Finnish-English edition. NMKL methods are avail-able through the office of the Secretary General and cost FIM 25 or US $ 6 each.

The address is: Nordie Committee on Food Analysis, c/o Technical Research Centre of Finland, Food Research Laboratory, SF-02150 ESBO, Finland. NMKL can be reached through telex: 122972 vttha sf or via telefax: +358-0-462382.

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Nordisk Metodikkommillé för Livsmedel Generalsekretariatet

NEW NMKl METHOOS

The following methods of analysfs for food have been published by the Nordie Committee on Food Analysis in 1988 and are

available through NMKL's office in Finland: Collaboratively Studied Chemical Methods

POSTADRESS

*

Histamine. Qualitative thin-layer chromatographic screening

method for fish (NI~KL no 118), 2nd ed.

NMKL no 118 (1988) replaces the first edition of the method,

which was published as a proposed method in 1986. The method

has now been collaboratively studied and is issued as an

official NMKL method. Benedicte Hald at the Royal Veterinary

and AgriciJltural University in Denmark, coordinated the

collaborative test. Twelve laboratories participated in the

collaborative study, which included 5 samples containing

histamine at levels from 0 mg/kg to 1000 mg/kg. At the lowest

tested level, 100 mg histamine/kg, eight laboratorfes found

from 60 to 250 mg histamine/kg while the rest of the

collaborators reported "less than 100 mg/kg". No laboratory

reported "not detected" or zero at this level. The method has

a sensitivity of 200 mg histamine/kg and a recovery of 90 % on

thi s 1 eve 1 •

The 'method can be applied to fish products and has only been

tested on such products. If it is intended to apply the method

to foods other than fish products, it should be noted that it

may be necessary to introduce rnodifications.

*

Tin. Determination by atomie absorption in fruits and

vegetables (NMKL no 126)

This collaboratively studied method is applicable to the

determination of tin in fruits and vegetables in the

concentration range 10 to 500 mg/kg. It is a rapid method,

especially suitable for routine determinations of tin in

canned fruits and vegetables contaminated with migrated tin

from the can. Rolando Mazzone, Erik Frandsen (PLM Haustrup,

Odense) and Knud Voldum-Clausen (National Food A9ency,

Copenhagen) from Denmark have each in turn contributed to the

elaboration, collaborative testing and final editing of this method.

TELEX

NORDISK METODIKKOMMITIE FÖR LIVSMEDEL

c/o Stalens tekniska forsknin9sccntral TELEFON Nat. (90) 4 561 Inl. +358-0-4561 122972 vtlha si BANKFÖABINDELSE POSTGIRO 2238-9 Livsmedelslaboratoriel SF-02150 ESBO, FINLAND

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Proposed 11ethod

( .

In the collaborative testing of the methad two samples of tomato suoup and two samples of dpple sauce were analyzed in 13 laboratories. The repeatability relative standard

deviations were 4.3 and 2.4 % in the tomato soup samples and 7.7 and 2.9 % in two samples of apple sauce. The corresponding parameters for reproducibility were 12.0 and 7.6 % for tomato soup and 9.4 and 4.0 % for apple sauce. The coordinators of the collaborative study are working on a report of the study, aiming at publishing it shortly in a scientific journal.

*

Hydroxyproline. Colorimetrie determination as a measure of

collagen ;n ~~eat and 11eat products (Nl~KL no 127)

This method, which describes the quantitative determination of hydroxyproline and an estimation of the amount of collageneus connective tissue in meat and meat products, has been

collaboratively studied in 18 laboratories. Eight samples were

included. (

Kurt Kol ar of the Swedi sh ~1eat Research Ins ti tute in Kävl i nge, Sweden, coordinated the study. The final report of the study is expected to be published soon. As determined in the col-laborative study, the within laboratory precision of the method, its repeatability, allows the hydroxyproline content of a sample containing the analyte at the 0.50 g/100 g level, to be determined with a precision of I 0.03 g/100 g. The

corresponding between laboratory parameter, the reproduci-bility of the method, prediets that results from different laboratories at the level 0.50 g hydroxyproline/100 g will vary within ±0.05g/100 g.

*

Polyphosphates. Detection by paper chromatography in meat products etc. (NMKL no 76, 2nd Ed)

NMKL no 76 (1988) replaces the first edition of no 76 published in 1970 and has been elaborated by Per Joner of the Non1egian College of Veterinary Medicine in Norway. It has been revised according to experiences of the Oslo Board of Health Dept of Food Control where ca 1000 polyphosphate determinations are performed each year. The methad has not been subjected toa full collaborative study and is there-fore published as an NMKL proposed method, not an NMKL method.

Compared to the first edition of this method, the following changes have been made:

1. For greater accuracy in reading of chromatogrammes and for increased sensitivity the developers have been changed.

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(45)

2. To reduce the consumption of trichloroacetic acid, which

is a toxic compound, the sample preparation has been

simplified: meat samples are extracted with warm water

only. It has been found, that the trichloroacetic acid

present in the chromatography solvent is sufficient to

achieve precipitation of proteins present in meats. Only

milk powder, caseinates and blood plasma samples are

extracted with 20 % trichloroacetic acid. For confirmation

of results meat samples found to be positive for

poly-phosphates when extracted with water are re-chromatographed after trichloroacetic acid extraction.

Microbiological Method

*

Pretreatment of foods for •icrobiological examination

(NMKL no 91, 2nd Ed)

NMKL no 91 (1988) replaces the first edition of the method published in 1975. This method describes a routine technique

for sampling and further pretreatment of samples for

subsequent determination of microorganisms. The method can be used with solid, semi-solid and liquid foods. In solid foods both surface flora and depth flora may be determined.

The method does not take into account obligatory anaerobic

Gram negative non-spore forming microorganisms. Mette Nyborg

and Bj~rn Fredebo Thomsen (Denmark) have been responsible

for the elaboration of these instructions.

Most microbiological NMKL methods include no pretreatment

instructions but contain a reference to NMKL no 91. Please

make sure that this new edition of the method for sampling

and further pretreatment is always used in conneetion with

microbiological NMKL-methods.

ORDERING Of METHOOS

All NMKL methods are published in a Scandinavian language

(Oanish, Danish, Norwegian or Swedish) and in English.

Since 1985 all new methods are also available in a

Finnish-English edition. NMKL methods cost FIM 25 or US$ 6 each

and are available through NMKL1

s office:

Nordie Committee on Food Analysis, c/o Technical Research

Centre of Finland, Food Research Laboratory, SF-02150 ESBO,

Finland. NMKL can also be reached through telex: 122972

(46)

(47)

lh~~

7·'1·

NORDIC COMMITTEE ON FOOD ANALYSIS

Nordisk Metodikkommitté för Livsmedel

Generalsekretariatet

NMKL COLLABORATIVE STUDIES PLANNED FOR 1988/89

Code No 3.10.3 3.12.1 3.20 8.11.6 12.3.4.2 ~lethod

Microbiological methods, automatization. DEFT-methods

Aflatoxin. Oetermination in peanuts and peanut prod~cts (Rev no 90)

Listeria monocytogenes. Detection in food

PCB. Congener specific determination in food

Starch. Enzymatic determination in

rneat products November 1988 Referee Flemming Boisen Miljö- og levnedsmiddel-kontrolenheden Mikrobiologisk Laboratorium

Lille Tornbjerg vej 24 DK-5220 ODENSE S0 DENMARK

lord l~öller

National Food Administration

Box 622

S-751 26 UPPSALA

SWEDEN

Professor Niels Skovgaard

Royal Veterinary and

Agricultural University Institute of Hygiene and

~1i crobi ol ogy

Bülowsvej' 13

OK-1870 FREDERIKSBERG DENMARK

Kimmo Himberg

Techn Res Centre of Finland Food Research Laboratory SF-02150 ESPOO

FINLAND

Or Ulla Edber~

National Food Administration

Box 62~

S-751 26 UPPSALA SWEDEN

POSTADRESS

c/o Stalens tekniska forskningscentral

TELEFON Nat. (90) 4561 TELEX 122972 vttha sf BANKFÖRBINDELSE POSTGIRO Livsmedelslaboratoriet SF-02150 ESBO. FINLAND Int. +358-Q-4561 2238-9

(48)

tWRDIC COt~f.UTTEE ON FOOD ANALYSIS (NMKL)

Nordisk Metodikkommitté för Livsmedel Generalsekretariatet

IO.o't

l

.",,~ '?.l.u

METHOOS UNDER DEVELOPMENT VITHIN THE NORDIC COMMITTEE ON FOOD ANALYSIS

Code No 3.2.1 3.5 3.8 3.10.3 3.12.1 3.17 Method

Coliform bacteria. Deter

-mination in foods (Rev no 44)

Fecal streptococci. Deter-mination in foods (Rev no 68) Salmonella bacteria. Detection in foods (Rev no 71, 3rd ed.) Microbiological methods, automatization. DEFT-methods Aflatoxin. Determination in peanuts and peanut products (Rev no 90) Campylobacter jejuni/coli. Detection in food ( Rev no 119) Referee Ivar Hellesnes Trondheim off. kj~tt- og naringsmiddelkontroll Bratt~ra N-7000 TRONDHEIM NORWAY Steen Ewald

Norwegian College of Veterinary Medicine, P.O.Box 8146 Dep.

N-0033 OSLO 1 NORWAY

Christer Wiberg

National Food Administration Box 622 S-751 26 UPPSALA SWEDEN Flemming Boisen Milj~- og levnedsmiddel-kontrolenheden Mikrobiologisk Laboratorium

L ill e Tornbj erg vej 24 DK-5220 ODENSE S0 DENMARK

Tard Möller

Natianal Faod Administratian Box 622

S-751 26 UPPSALA S\4EDEN

Mats Peterz

Natianal Faad Adrninistration Box 622

November 1988

Status

Revi sed methad being drafted

Rev i sed met ho d being drafted

Revised methad being drafted

New draft methad to be collabor-atively studied in 1988/89 Collabarative study schedul ed for winter 1988/89 Collaborative study of revi sed method completed Report expected befare 1.12.1988 POSTADRESS

NORDISK METOOIKKOMMITIE FÖR LIVSMEDEL

cto Slalens tekniska forskningscentral

TELEFON Nat. (90) 4561 TELEX t 22972 vttha sf BANKFÖABINDELSE POSTGIRO Livsmedelslaboraloriet SF-02 t 50 ESBO, FINLAND Int. +358-0-4561 2238-9

(49)

8.6.10.3 Su1fite. Spectrophotometric determination in food

8.6.10.4 Su1fite. Enzymatic determination in food

8.9.3.2.1 Betacarotene, beta-apo-8

-carotenal and canthaxantin. Determination by HPLC in food 8.11.6 PCB. Congener specific determination in food 8.13 Metals. Determination by atomie absorption

~.16.2 G1utamic acid and monosodium

g1utamate. Enzymatic deter-mination in meat and fish products and in soups

Eva Lönberg

Nat i on a 1 Food-Admi ni strati on Box 622

Dr U11a Edberg

National Food Administration Box 622

Dr Tapani Suortti

FINLAND

Kimmo Himberg

FINLAND Lars Jorhem

National Food Administration Box 622

Tapani Hattula

Techn Res Centre of Finland 1

Food Research Laboratory SF -02150 ESPOO

FINLAND

Collaborative s tudy comp 1 eted. Report under consideration Collaborative study completed Report under consideration Collaborative s tudy comp 1 eted Report expected before 1.12.198 Joint NMKL/AOAC Collaborative study scheduled for 1988/89 Collaborative study schedul ed for autumn 1988 Collaborative study schedul er. for autumn 1988 12.3.1/

12.3.2 Water and ash. Gravimetrie determination in meat products Statens Teknologiske Britt Hanto

Revised method Institutt being drafted

12.3.3

(Rev no 23, 2nd ed.) Postboks 8116, Dep.

Fat. Oetermination after SBR in meat and meat products (Rev no 88)

N-0032 OSLO 1

NORWAY

Lars-Börje Croon

National Food Administration Box 622 S-751 26 UPPSALA SHEDEN Collaborative study of preser and revised method complet• Report expecte' before 1.12.19·